RF (Resorcinol-Formaldehyde) aerogels and carbon aerogels were prepared through the sol-gel method following the routes of polymerization, gelation, supercritical drying and pyrolysis processes. The influence of fabrication parameters on the textural structure of the samples, e.g., specific surface area, pore size, and pore size distribution, etc., were systematically investigated. With a decrease in the R/F molar ratio, or an increase in the catalyst content within a limited range, the porosity of the nanostructure materials increases. The optimal temperature of pyrolysis for RF aerogel was investigated by TGA (Thermogravimetric Analysis).